UPLC-MS/MS检测猪肉中硝基呋喃类药物残留方法的优化

Optimization of methods for determination of nitrofuran residues in pork by UPLC-MS/MS

[目的]为了解猪肉中硝基呋喃类药物残留的情况,并对所选方法进行优化。[方法]按UPLC-MS/MS法进行优化检测猪肉中呋喃它酮(FTD)、呋喃唑酮(FZD)、呋喃西林(NFZ)和呋喃妥因(NFT)残留量,用甲醇洗涤样品,使用10%三氯乙酸创造酸性条件,使样品与2-硝基苯甲醛发生衍生化反应,同时可以更有效地沉淀蛋白质,以减少蛋白质对于试验的干扰。衍生化完成后用乙酸乙酯提取2次,用正己烷除去脂肪。以乙腈0.1%的甲酸和0.5 mmol/m L醋酸铵混合水溶液为流动相,在ESI的正离子模式下进行扫描,检测模式采用多反应监测(MRM)。[结果]通过该方法检测的硝基呋喃类药物为1~100 ng/mL时具有良好的线性关系,检测下限均为0.3μg/kg,平均回收率为91.0%~117.8%,平均相对标准差RSD为2.9%~7.3%,满足国家标准要求。[结论]该方法具有净化效果好、灵敏度高、结果稳定等优点,能够较方便准确地检测出市场猪肉中硝基呋喃类药物的残留。

[Objectives]In order to understand the situation of nitrofuran residues in pork,optimized the selected method.[Methods]There residues of furaltadone(FTD),furazolidone(FZD),furacilin(NFZ)and furantoin(NFT)in pork were optimized by UPLC-MS/MS method.The samples were washed with methanol,and 10%trichloroacetic acid was used to create acidic conditions,so that the samples could be derivatized with 2-nitrobenzaldehyde,and protein could be precipitated more effectively to reduce the interference of protein to the experiment.After derivatization,extracted it twice with ethyl acetate,and removed the fat with n-hexane.The mobile phase was the mixed aqueous solution of acetonitrile 0.1%formic acid and 0.5 mmol/mL ammonium acetate,which was scanned in the positive ion mode of ESI.The detection mode was multiple reaction monitoring(MRM).[Results]The nitrofurans detected by this method had a good linear relationship between 1-100 ng/mL.The detection lower limit was 0.3μg/kg,the average recovery was 91.0%-117.8%,and the average relative standard deviation(RSD)was 2.9%-7.3%,meeting the national standard requirements.[Conclusions]The method has the advantages of good purification effect,high sensitivity and stable results,and could be used to detect nitrofurans residues in market pork conveniently and accurately.